FR2633641A1 - PROCESS AND DEVICE FOR THE SIMULTANEOUS PROTECTION OF INTERNAL AND EXTERNAL SURFACES, PARTICULARLY BY ALUMINIZATION OF HOT-RESISTANT ALLOY PARTS, BASED ON NI, CO OR FE - Google Patents

PROCESS AND DEVICE FOR THE SIMULTANEOUS PROTECTION OF INTERNAL AND EXTERNAL SURFACES, PARTICULARLY BY ALUMINIZATION OF HOT-RESISTANT ALLOY PARTS, BASED ON NI, CO OR FE Download PDF

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Publication number
FR2633641A1
FR2633641A1 FR8808801A FR8808801A FR2633641A1 FR 2633641 A1 FR2633641 A1 FR 2633641A1 FR 8808801 A FR8808801 A FR 8808801A FR 8808801 A FR8808801 A FR 8808801A FR 2633641 A1 FR2633641 A1 FR 2633641A1
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France
Prior art keywords
box
parts
coated
donor
external
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Granted
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FR8808801A
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French (fr)
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FR2633641B1 (en
Inventor
Jean-Paul Fournes
Rene Jean Morbioli
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Safran Aircraft Engines SAS
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SNECMA SAS
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Publication date
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Priority to FR8808801A priority Critical patent/FR2633641B1/en
Priority to IL90775A priority patent/IL90775A/en
Priority to EP89401841A priority patent/EP0349420B1/en
Priority to DE8989401841T priority patent/DE68902284T2/en
Priority to CA000604433A priority patent/CA1338587C/en
Priority to US07/372,889 priority patent/US5068127A/en
Publication of FR2633641A1 publication Critical patent/FR2633641A1/en
Priority to US07/763,220 priority patent/US5149376A/en
Application granted granted Critical
Publication of FR2633641B1 publication Critical patent/FR2633641B1/en
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    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/04—Coating on selected surface areas, e.g. using masks
    • C23C16/045—Coating cavities or hollow spaces, e.g. interior of tubes; Infiltration of porous substrates
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C10/00—Solid state diffusion of only metal elements or silicon into metallic material surfaces
    • C23C10/02—Pretreatment of the material to be coated
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C10/00—Solid state diffusion of only metal elements or silicon into metallic material surfaces
    • C23C10/06—Solid state diffusion of only metal elements or silicon into metallic material surfaces using gases
    • C23C10/08—Solid state diffusion of only metal elements or silicon into metallic material surfaces using gases only one element being diffused
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C10/00—Solid state diffusion of only metal elements or silicon into metallic material surfaces
    • C23C10/06—Solid state diffusion of only metal elements or silicon into metallic material surfaces using gases
    • C23C10/14—Solid state diffusion of only metal elements or silicon into metallic material surfaces using gases more than one element being diffused in one step
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/06—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of metallic material
    • C23C16/08—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of metallic material from metal halides
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/06—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of metallic material
    • C23C16/08—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of metallic material from metal halides
    • C23C16/12—Deposition of aluminium only
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
    • C23C16/448—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating characterised by the method used for generating reactive gas streams, e.g. by evaporation or sublimation of precursor materials
    • C23C16/4488—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating characterised by the method used for generating reactive gas streams, e.g. by evaporation or sublimation of precursor materials by in situ generation of reactive gas by chemical or electrochemical reaction
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02T—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO TRANSPORTATION
    • Y02T50/00—Aeronautics or air transport
    • Y02T50/60—Efficient propulsion technologies, e.g. for aircraft

Landscapes

  • Chemical & Material Sciences (AREA)
  • Metallurgy (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Organic Chemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Electrochemistry (AREA)
  • Other Surface Treatments For Metallic Materials (AREA)
  • Chemical Vapour Deposition (AREA)
  • Physical Vapour Deposition (AREA)
  • Turbine Rotor Nozzle Sealing (AREA)

Abstract

Les pièces à revêtir 10a, 10b, 10c sont chauffées à une température supérieure à 1 000 degre(s)C dans une boîte 1 contenant en outre, et de manière séparée, un corps donneur 9 sous forme de granules comportant le métal à déposer et un corps 5 composé au moins de poudre anhydre de fluorure de chrome F3 Cr constituant un activateur, source de fluor. Un débit contrôlé d'un gaz porteur, réducteur ou neutre, est introduit 4 dans la boîte de manière à établir une circulation dans la boîte des vapeurs fluorées 13 obtenues, après décomposition thermique de F3 Cr et formation de fluorure volatil à partir du donneur. Un dispositif de mise en oeuvre du procédé est également décrit.The parts to be coated 10a, 10b, 10c are heated to a temperature above 1000 degree (s) C in a box 1 further containing, and separately, a donor body 9 in the form of granules comprising the metal to be deposited and a body 5 composed at least of anhydrous powder of chromium fluoride F3 Cr constituting an activator, a source of fluorine. A controlled flow rate of a carrier gas, reducing or neutral, is introduced 4 into the box so as to establish a circulation in the box of the fluorinated vapors 13 obtained, after thermal decomposition of F3 Cr and formation of volatile fluoride from the donor. A device for implementing the method is also described.

Description

DESCRIPTIONDESCRIPTION

L'invention concerne un procédé de dépôt simultané d'un revêtement protecteur, notamment à base d'aluminium, à la fois sur les surfaces externes et internes de pièces en alliages résistant à chaud, notamment à base de nickel, cobalt ou fer. Elle concerne également un dispositif  The invention relates to a method of simultaneously depositing a protective coating, in particular based on aluminum, both on the external and internal surfaces of parts made of heat-resistant alloys, in particular based on nickel, cobalt or iron. It also relates to a device

adapté à la mise en oeuvre dudit procédé.  suitable for implementing said method.

FR-A-1 433 497 décrit un procédé d'aluminisation en phase vapeur selon lequel l'aluminium déposé est transféré sans contact solide-solide entre le donneur contenant le métal à déposer et la pièce à revêtir, le donneur réagissant  FR-A-1 433 497 describes a vapor phase aluminization process in which the deposited aluminum is transferred without solid-solid contact between the donor containing the metal to be deposited and the part to be coated, the donor reacting

avec un halogénure, notamment un fluorure.  with a halide, in particular a fluoride.

D'autres procédés plus récents, dont un exemple est fourni par US-A-4 132 816 et US-A-4 148 275, proposent une solution pour obtenir une protection améliorée des surfaces internes de pièces creuses, notamment des aubes de turbine refroidies présentant des circuits internes, fins et complexes. Aucun de ces procédés connus ne donne toutefois entière satisfaction. Notamment US-A- 4 132 816 et US-A- 4 148 275 imposent des modalités complexes de mise en oeuvre utilisant des boites à deux compartiments et deux sources distinctes de donneur lorsqu'on doit réaliser une protection à la fois sur des surfaces  Other more recent methods, an example of which is provided by US-A-4,132,816 and US-A-4,148,275, provide a solution for obtaining improved protection of the internal surfaces of hollow parts, in particular cooled turbine blades. with fine, complex internal circuits. None of these known methods is entirely satisfactory, however. In particular US-A-4,132,816 and US-A-4,148,275 impose complex methods of implementation using boxes with two compartments and two distinct sources of donor when protection must be provided both on surfaces

externes et sur des surfaces internes de pièces.  external and internal surfaces of parts.

Des résultats améliorés et une simplification de la mise en oeuvre sont obtenus par le procédé consistant - (a) à chauffer à une température supérieure à 1000*C une botte contenant les pièces à revêtir et, de manière séparée, un corps constituant le donneur du métal à déposer, notamment l'aluminium et  Improved results and a simplification of the implementation are obtained by the process consisting of - (a) heating at a temperature above 1000 ° C. a boot containing the parts to be coated and, separately, a body constituting the donor of the metal to be deposited, in particular aluminum and

2 L;26336412 L; 2633641

notamment sous forme de granules et un corps consti-  especially in the form of granules and a body

tuant un activateur, composé au moins de fluorure de chrome, F3 Cr, sous forme de poudre anhydre constituant une source de fluor - (b) à établir une circulation dans la boite des vapeurs fluorées obtenues, d'une part après décomposition thermique de F3 Cr et d'autre part, comportant le fluorure volatil après passage sur ledit donneur, notamment F3 Al, en introduisant dans ladite boite un débit contrôlé d'un gaz porteur réducteur ou neutre, notamment argon, de manière à obtenir par le contact desdites vapeurs métallisées avec les surfaces externes et internes des pièces un  killing an activator, composed at least of chromium fluoride, F3 Cr, in the form of an anhydrous powder constituting a source of fluorine - (b) to establish a circulation in the box of the fluorinated vapors obtained, on the one hand after thermal decomposition of F3 Cr and on the other hand, comprising the volatile fluoride after passage over said donor, in particular F3 Al, by introducing into said box a controlled flow rate of a reducing or neutral carrier gas, in particular argon, so as to obtain by contact with said vapors metallized with the external and internal surfaces of the parts a

revêtement protecteur, notamment une aluminisation.  protective coating, in particular aluminization.

Avantageusement, avant l'application dudit procédé  Advantageously, before the application of said method

conforme à l'invention, une étape antérieure peut per-  according to the invention, an earlier step can

mettre d'effectuer un revêtement préalable, notamment des surfaces externes des pièces à revêtir, notamment à base de Cr, Pt ou dépôt complexe de type M Cr A1 Y, obtenu par  put to perform a prior coating, in particular of the external surfaces of the parts to be coated, in particular based on Cr, Pt or complex deposit of type M Cr A1 Y, obtained by

tout procédé connu en soi.any process known per se.

Un dispositif adapté à la mise en oeuvre dudit procédé conforme à l'invention se compose d'une boite placée dans une enceinte susceptible d'être chauffée et remplie d'un gaz protecteur de type argon, éventuellement soumis à un débit contrôlé de circulation. Ladite boite comporte, à sa partie inférieure, une rampe, raccordée à une alimentation externe sous débit contrôlé, de distribution d'un gaz porteur réducteur ou neutre, par exemple argon. Au-dessus, la boîte comporte des grillessupports portant d'une part,  A device adapted to the implementation of said method according to the invention consists of a box placed in an enclosure capable of being heated and filled with a protective gas of argon type, possibly subject to a controlled flow of circulation. Said box comprises, at its lower part, a ramp, connected to an external power supply under controlled flow, for the distribution of a reducing or neutral carrier gas, for example argon. Above, the box has support grids bearing on the one hand,

de la poudre de fluorure de chrome F3 Cr anhydre, éven-  anhydrous F3 Cr chromium fluoride powder, even

tuellement mélangée à un support inerte de type A1203 et d'autre part, un donneur solide sous forme de  tually mixed with an inert support of the A1203 type and on the other hand, a solid donor in the form of

3 26336413 2633641

granules d'un alliage du métal à déposer, notamment alu-  granules of an alloy of the metal to be deposited, in particular aluminum

minium. A la partie supérieure de la boite, sont placées les pièces à revêtir, les orifices de. sortie des circuits internes des pièces étant tournés vers l'admission du flux de la phase gazeuse circulant dans la boite. Selon l'effet recherché, les pièces sont entièrement immergées dans la boite ou des parties non revêtues sont disposées à  minimum. At the upper part of the box, are placed the parts to be coated, the orifices. output of the internal circuits of the parts being turned towards the admission of the flow of the gaseous phase circulating in the box. Depending on the desired effect, the parts are fully immersed in the box or uncoated parts are arranged at

l'extérieur de la boîte et sont, éventuellement, recou-  outside of the box and are possibly covered

vertes d'un cache.green of a cache.

D'autres caractéristiques et avantages de l'invention  Other characteristics and advantages of the invention

seront mieux compris à la lecture de la description qui va  will be better understood on reading the description which will

suivre d'un exemple de réalisation du procédé conforme à l'invention et d'un dispositif de mise en oeuvre dudit procédé, en référence au dessin annexé sur lequel: - la figure 1 représente une vue schématique en coupe axiale d'une boîte destinée à la mise en oeuvre du procédé de dépôt simultané d'un revêtement protecteur à la fois sur les surfaces externes et internes de  follow of an embodiment of the method according to the invention and of a device for implementing said method, with reference to the attached drawing in which: - Figure 1 shows a schematic view in axial section of a box intended to the implementation of the process of simultaneously depositing a protective coating on both the external and internal surfaces of

pièces en alliages résistant à chaud.  parts made of heat resistant alloys.

Dans certaines applications des pièces en alliages résistant à chaud, à base de Ni, Co ou Fe, notamment aux moteurs aéronautiques, il est souvent nécessaire de concilier de bornnes caractéristiques de tenue mécanique  In certain applications of parts made of heat-resistant alloys, based on Ni, Co or Fe, in particular for aeronautical engines, it is often necessary to reconcile terminal blocks with mechanical properties

à chaud et de tenue aux agressions provenant de l'envi-  hot and resistant to attacks from the environment

ronnement sous forme d'oxydation ou de corrosion de divers agents. Ces exigences conduisent à prévoir sur ce type de pièces un revêtement protecteur. Un procédé couramment utilisé selon FR-A-l 433 497 de dépôt en phase vapeur s'est révélé inefficace lorsqu'il s'agit d'étendre ce dépôt protecteur sur les surfaces internes de pièces complexes dont des exemples d'applications sur moteurs aéronautiques sont fournis par des rampes de distribution  reason in the form of oxidation or corrosion of various agents. These requirements lead to providing a protective coating on this type of part. A process commonly used according to FR-Al 433 497 for vapor deposition has been shown to be ineffective when it comes to extending this protective deposition on the internal surfaces of complex parts of which examples of applications on aeronautical engines are provided. by distribution ramps

4 26336414 2633641

de carburant ou par des aubes refroidies de turbine comportant des circuits internes, fins et complexes. Le procédé conforme à l'invention permet d'obtenir le dépât simultané d'un revêtement protecteur & la fois sur les surfaces externes et les surfaces internes de ce type de pièces, dans des conditions facilitant la mise en oeuvre  fuel or by cooled turbine blades with internal, fine and complex circuits. The method according to the invention makes it possible to obtain the simultaneous damage of a protective coating & both on the external surfaces and the internal surfaces of this type of part, under conditions facilitating the implementation.

tout en assurant l'obtention de résultats satisfaisants.  while ensuring satisfactory results.

Le dispositif de mise en oeuvre représenté schématiquement à la figure 1 comporte une boite 1 munie d'un couvercle 2 coopérant au niveau d'un rebord 3. Cette boite 1 est placée dans une enceinte de traitement de tout type connu dans une atmosphère protectrice, par exemple sous argon, ladite enceinte étant équipée de moyens de chauffage, notamment électriques. A la partie inférieure de la boite 1 est placée une rampe 4 raccordée à un moyen externe de tout type connu d'alimentation en gaz porteur qui peut être de type réducteur ou neutre, par exemple et de  The implementation device shown diagrammatically in FIG. 1 comprises a box 1 provided with a cover 2 cooperating at the level of a flange 3. This box 1 is placed in a treatment enclosure of any known type in a protective atmosphere, for example under argon, said enclosure being equipped with heating means, in particular electric. At the lower part of the box 1 is placed a ramp 4 connected to an external means of any known type of carrier gas supply which can be of reducing or neutral type, for example and of

préférence de l'argon. L'arrivée à la rampe de distri-  preferably argon. Arrival at the distribution ramp

bution 4 est munie d'un moyen connu de réglage du débit de gaz, par exemple une vanne. Le réglage de ce débit tient compte du volume de la boîte 1, de son taux de remplissage en pièces à revêtir et peut éventuellement  bution 4 is provided with a known means for adjusting the gas flow rate, for example a valve. The adjustment of this flow rate takes account of the volume of the box 1, of its filling rate with parts to be coated and may possibly

être déterminé par un essai simple à réaliser, une circu-  be determined by a simple test to perform, a circu-

lation suffisante correspondant à la qualité recherchée du revêtement obtenu. Au-dessus, est disposé un lit 5 de fluorure de chrome F3 Cr, sous forme de poudre anhydre, éventuellement mélangée à un support inerte de type A12 03, placé par exemple dans des coupelles 6  sufficient lation corresponding to the desired quality of the coating obtained. Above is a bed 5 of chromium fluoride F3 Cr, in the form of anhydrous powder, optionally mixed with an inert support of type A12 03, placed for example in cups 6

posées sur une grille-support 7. Une grille-support supé-  placed on a support grid 7. An upper support grid

rieure 8 porte un donneur 9 grossièrement concassé, par exemple sous forme de granules de dimensions supérieures à quatre millimètres et qui peut être, lorsque le métal à déposer est l'aluminium, en un alliage de type CA 30, à  lower 8 carries a coarsely crushed donor 9, for example in the form of granules of dimensions greater than four millimeters and which can be, when the metal to be deposited is aluminum, in an alloy of type CA 30, with

70% Cr et 30% Al, en pourcentages pondéraux de composition.  70% Cr and 30% Al, in percentages by weight of composition.

A la partie supérieure de la boite 1, sont disposées les pièces 10 à revêtir. Lorsqu'une protection complète de la pièce est recherchée, les pièces, telles que 10a représentée à la figure 1, sont complètement immergées dans la botte 1 et peuvent être suspendues par tout moyen connu, par exemple un support 11 dans lequel est ménagé un passage permettant la circulation du gaz de l'intérieur de la pièce vers l'extérieur de la boite. Le support 11 peut  At the upper part of the box 1, are arranged the pieces 10 to be coated. When complete protection of the part is sought, the parts, such as 10a shown in FIG. 1, are completely immersed in the boot 1 and can be suspended by any known means, for example a support 11 in which a passage is made. allowing the circulation of gas from inside the room to the outside of the box. Support 11 can

notamment être constitué par un tube. Lorsqu'une pro-  in particular be constituted by a tube. When a pro-

tection est prévue avec épargne, la partie non revêtue est maintenue à l'extérieur de la boite 1, comme dans le cas des pièces 10b et 10c représentées à la figure 1, traversant des passages 2a ménagés sur le couvercle 2 de la boite 1. Un cache tel que 12 peut être utilisé pour masquer la partie de pièce non revêtue. Dans certains cas, une circulation externe à faible débit du gaz protecteur suffit pour que le courant de gaz non réactif créé autour de la. partie non revêtue, par exemple de la pièce 10b,  tection is provided sparingly, the uncoated part is kept outside of the box 1, as in the case of the parts 10b and 10c shown in FIG. 1, passing through passages 2a formed on the cover 2 of the box 1. A cover such as 12 can be used to hide the uncoated part. In some cases, an external circulation at low flow rate of the protective gas is sufficient for the stream of non-reactive gas created around the. uncoated part, for example of part 10b,

empêche tout dépôt sur cette partie.  prevents any deposit on this part.

Le procédé de protection conforme à l'invention utilisant un dispositif du type qui vient d'être décrit se déroule  The protection method according to the invention using a device of the type which has just been described takes place

de la manière ci-après décrite.as described below.

L'enceinte de traitement contenant la boite 1 est portée à une température supérieure à 1000 C, à une vitesse de montée approximative de 17'C par minute. Une température de maintien courament utilisée selon l'inventionet donnant des résultats satisfaisants est de 1150C. A cette température, la décomposition thermique du fluorure de chrome F3 Cr utilisé est lente, progressive et constante. En fonction des volumes respectifs en présence, la présence d'A12 03 peut éventuellement modérer le débit des vapeurs fluorées obtenues. Sous l'influence du courant d'argon débité dans la boite 1, il se produit à partir de ce moment, un balayage continu du donneur 9 qui fournit du fluorure d'aluminium très volatil, puis, des pièces 10 à revêtir, la circulation se faisant notamment à l'intérieur desdites pièces 10, de manière régulière et continue durant le temps de maintien du traitement. Pour une température de 1150C, un temps de maintien de deux heures est généralement suffisant. Des températures et des temps de maintien différents peuvent être utilisés et ces paramètres sont aisément déterminés d'après les résultats satisfaisantsobtenus lors d'un essai préalable, en fonction des paramètres de traitements connus pour l'alliage constituant les pièces à traiter. Les superalliages, notamment à base de Ni, Co ou Fe, couramment utilisés dans les applications sur pièces de moteurs aéronautiques conduisent généralement à adopter des températures comprises entre 1050'C et 1150'C et des  The treatment chamber containing the box 1 is brought to a temperature above 1000 ° C., at an approximate rise speed of 17 ° C. per minute. A holding temperature commonly used according to the invention and giving satisfactory results is 1150C. At this temperature, the thermal decomposition of the chromium fluoride F3 Cr used is slow, progressive and constant. Depending on the respective volumes present, the presence of A12 03 may possibly moderate the flow of fluorinated vapors obtained. Under the influence of the argon current delivered in the box 1, there occurs from this moment, a continuous scanning of the donor 9 which provides very volatile aluminum fluoride, then, of the parts 10 to be coated, the circulation taking place in particular inside said parts 10, in a regular and continuous manner during the treatment maintenance time. For a temperature of 1150C, a holding time of two hours is generally sufficient. Different temperatures and holding times can be used and these parameters are easily determined from the satisfactory results obtained during a prior test, as a function of the known treatment parameters for the alloy constituting the parts to be treated. Superalloys, in particular based on Ni, Co or Fe, commonly used in applications on parts of aeronautical engines generally lead to the adoption of temperatures between 1050 ° C. and 1150 ° C. and

temps de maintien compris entre deux et cinq heures.  holding time between two and five hours.

Dans l'exemple d'aubes 10 représentées à la figure 1, le courant gazeux symbolisé par les flèches 13 est en contact avec la paroi extérieure des aubes et traverse les circuits internes de refroidissement de l'aube en pénétrant par les évents et les orifices ménagés sur/bords et les parois de l'aube et en sortant par l'ouverture ménagée au niveau du pied de l'aube. La réaction bien connue, notamment par FR-A-1 433 497, d'aluminisation des surfaces par F3 Ai, avec dép6t et diffusion d'aluminium se produit ainsi, créant le revêtement protecteur  In the example of blades 10 shown in FIG. 1, the gas current symbolized by the arrows 13 is in contact with the outer wall of the blades and passes through the internal cooling circuits of the blade by penetrating through the vents and the orifices. formed on / edges and the walls of the blade and leaving through the opening formed at the foot of the blade. The well-known reaction, in particular by FR-A-1 433 497, of aluminizing surfaces with F3 Ai, with deposit and diffusion of aluminum thus occurs, creating the protective coating

recherché.research.

Le procédé de protection conforme à l'invention qui vient d'être décrit présente en outre l'avantage de pouvoir être associé sans modification des conditions de mise en oeuvre  The protection method according to the invention which has just been described has the further advantage of being able to be combined without modifying the conditions of implementation.

à un procédé global plus complexe de protection de pièces.  to a more complex overall process for protecting parts.

En effet, une étape préalable peut être effectuée, permettant de réaliser par tout procédé connu, un dépôt de Cr, Pt ou d'un alliage de type M Cr A1Y qui est notamment appliqué sur les surfaces externes des pièces, cette  Indeed, a preliminary step can be carried out, making it possible by any known method, to deposit Cr, Pt or an alloy of the M Cr A1Y type which is in particular applied to the external surfaces of the parts, this

étape étant suivie d'une protection réalisée selon l'in-  step followed by protection carried out according to the

vention, notamment une aluminisation.  vention, in particular aluminization.

Claims (5)

REVENDICATIONS 1. Procédé de dépôt simultané d'un revêtement protecteur, notamment à base d'aluminium, à la fois sur les surfaces externes et internes de pièces en alliages résistant à chaud, notamment à base de Ni, Co, Fe caractérisé en ce qu'il consiste: - (a) A chauffer à une température supérieure A lO1000C une boite contenant les pièces à revêtir et, de manière séparée, un corps constituant le donneur du métal A déposer.,. notamment l'aluminium et notamment sous forme de granules et un corps constituant un activateur, composéau moins de fluorure de chrome F3 Cr, sous forme de poudre anhydre, constituant une source de fluor; - (b) A établir une circulation dans la boite des vapeurs fluorées obtenues, d'une part après décomposition thermique de F3 Cr et, d'autre part, comportant le fluorure volatil obtenu après passage sur ledit donneur, notamment F3 Al, en introduisant dans la boîte un débit contr5ôlé d'un gaz porteur réducteur ou neutre, notamment argon, de manière A obtenir, par le contact desdites vapeurs métallisées avec les surfaces externes et internes des pièces, un  1. Process for the simultaneous deposition of a protective coating, in particular based on aluminum, both on the external and internal surfaces of parts made of heat-resistant alloys, in particular based on Ni, Co, Fe, characterized in that it consists of: - (a) Heating to a temperature above lO1000C a box containing the parts to be coated and, separately, a body constituting the donor of the metal to be deposited.,. in particular aluminum and in particular in the form of granules and a body constituting an activator, composed at least of chromium fluoride F3 Cr, in the form of anhydrous powder, constituting a source of fluorine; - (b) To establish a circulation in the box of fluorinated vapors obtained, on the one hand after thermal decomposition of F3 Cr and, on the other hand, comprising the volatile fluoride obtained after passage over said donor, in particular F3 Al, by introducing in the box a controlled flow of a reducing or neutral carrier gas, in particular argon, so as to obtain, by contact of said metallized vapors with the external and internal surfaces of the parts, a revêtement protecteur, notamment une aluminisation.  protective coating, in particular aluminization. 2. Procédé selon la revendication 1 dans lequel la tempé-  2. Method according to claim 1 wherein the temperature rature de traitement est comprise entre 1050 et 1150C  treatment scale is between 1050 and 1150C et sa durée est comprise entre 2 et 5 heures.  and its duration is between 2 and 5 hours. 3. Procédé selon l'une des revendications 1 ou 2 dans  3. Method according to one of claims 1 or 2 in lequel une étape préalable comporte l'obtention, par tout procédé connu en soi, d'un revêtement préalable A base de Cr, Pt ou d'un alliage complexe de type M Cr Ai Y,  which a prior step involves obtaining, by any process known per se, a prior coating based on Cr, Pt or a complex alloy of the M Cr Ai Y type, notamment sur les surfaces externes des pièces A revêtir.  especially on the external surfaces of the parts to be coated. 4. Dispositif de traitement destiné à la mise en oeuvre du  4. Processing device intended for the implementation of the procédé conforme A l'une des revendications 1 ou 2  process according to either of Claims 1 or 2 caractérisé en ce qu'il se compose d'une boite (1) placée dans une enceinte de traitement sous gaz protecteur, connue en soi, et comportant, à sa partie inférieure, une rampe (4), raccordée à une alimentation externe sous débit contrôlé, de distribution d'un gaz porteur réducteur ou  characterized in that it consists of a box (1) placed in a protective gas treatment enclosure, known per se, and comprising, at its lower part, a ramp (4), connected to an external power supply under flow controlled, distribution of a reducing carrier gas or neutre, notamment argon, surmontée d'une première grille-  neutral, notably argon, surmounted by a first grid- support (7) portant de la poudre de fluorure de chrome F3 Cr puis d'une deuxième grille-support (8) portant un donneur, notamment sous forme de granules d'un alliage du métal à déposer et à sa partie supérieure, les pièces à revêtir disposées de manière à orienter les orifices de sortie de leurs surfaces internes vers  support (7) carrying chromium fluoride powder F3 Cr then a second support grid (8) carrying a donor, in particular in the form of granules of an alloy of the metal to be deposited and at its upper part, the parts to be coated arranged so as to orient the outlet orifices of their internal surfaces towards l'admission du courant gazeux en circulation.  the admission of the gaseous current in circulation. 5. Dispositif de traitement selon la revendication 4 dans lequel la boîte (1) comporte les aménagements (2a) permettant de disposer A l'extérieur de ladite boite (1) fes parties de pièces non revêtues à-l'issue du traitement.  5. Treatment device according to claim 4 wherein the box (1) comprises the arrangements (2a) making it possible to have outside of said box (1) parts of parts not coated at the end of the treatment.
FR8808801A 1988-06-30 1988-06-30 METHOD AND DEVICE FOR THE SIMULTANEOUS PROTECTION OF INTERNAL AND EXTERNAL SURFACES, IN PARTICULAR BY ALUMINIZING HOT-RESISTANT ALLOY PARTS, BASED ON NI, CO OR FE Expired - Fee Related FR2633641B1 (en)

Priority Applications (7)

Application Number Priority Date Filing Date Title
FR8808801A FR2633641B1 (en) 1988-06-30 1988-06-30 METHOD AND DEVICE FOR THE SIMULTANEOUS PROTECTION OF INTERNAL AND EXTERNAL SURFACES, IN PARTICULAR BY ALUMINIZING HOT-RESISTANT ALLOY PARTS, BASED ON NI, CO OR FE
EP89401841A EP0349420B1 (en) 1988-06-30 1989-06-28 Process and apparatus for the simultaneous protection of both internal and external surfaces, especially by aluminising parts made of heat-resistant alloys based on ni, co or fe
DE8989401841T DE68902284T2 (en) 1988-06-30 1989-06-28 METHOD AND DEVICE FOR SIMULTANEOUS PROTECTION OF THE INTERNAL AND EXTERIOR SURFACES, ESPECIALLY IN THE ALUMINATION OF PARTS FROM HEAT-RESISTANT ALLOYS BASED ON NI, CO OR FE.
IL90775A IL90775A (en) 1988-06-30 1989-06-28 Process and apparatus for the simultaneous deposition of a protective coating on internal and external surfaces of heat- resistant alloy parts
CA000604433A CA1338587C (en) 1988-06-30 1989-06-29 Device and process for simultaneously protecting internal and external surfaces, such as by aluminization of thermoresistant ni, co or fe based alloy pieces
US07/372,889 US5068127A (en) 1988-06-30 1989-06-29 Process and apparatus for the simultaneous deposition of a protective coating on internal and external surfaces of heat-resistant alloy parts
US07/763,220 US5149376A (en) 1988-06-30 1991-09-20 Process and apparatus for the simultaneous deposition of a protective coating on internal and external surfaces of heat-resistant alloy parts

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
FR8808801A FR2633641B1 (en) 1988-06-30 1988-06-30 METHOD AND DEVICE FOR THE SIMULTANEOUS PROTECTION OF INTERNAL AND EXTERNAL SURFACES, IN PARTICULAR BY ALUMINIZING HOT-RESISTANT ALLOY PARTS, BASED ON NI, CO OR FE

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IL90775A (en) 1993-05-13
FR2633641B1 (en) 1993-02-05
CA1338587C (en) 1996-09-10
US5068127A (en) 1991-11-26
IL90775A0 (en) 1990-01-18
EP0349420B1 (en) 1992-07-29
EP0349420A1 (en) 1990-01-03
DE68902284D1 (en) 1992-09-03

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